反应详情

A mixture of 2-(3-methoxyphenyl)-6-phenyl-1H-imidazo[4,5-b]pyridine (Compound of Example 1) (80 mg), 2-tert-butylimino-2-diethylamino-1,3-dimethylperhydro-1,3,2-diazaphosphorine resin (PS-BEMP, 2.2 mmol/g) (181 mg) and N,N-dimethyl formamide (3.2 ml) was shaken at room temperature for 1 hour. To the mixture was added 4-fluorobenzyl chloride (46 mg), and the mixture was further shaken at room temperature for 15 hours. The resin was filtered off, and the filtrate was concentrated under reduced pressure. The residue was subjected to a preparative HPLC, and the desired fraction was concentrated. The concentrate was distributed into dichloromethane and a saturated aqueous solution of sodium bicarbonate. The organic layer was filtered by means of a PTFE filter tube, and concentrated under reduced pressure to obtain 1-(4-fluorobenzyl)-2-(3-methoxyphenyl)-6-phenyl-1H-imidazo[4,5-b]pyridine (84 mg, 78%).

1. stirringthe mixture was further shaken at room temperature for 15 hours
2. filtrationThe resin was filtered off
3. concentrationthe filtrate was concentrated under reduced pressure
4. concentrationthe desired fraction was concentrated
5. filtrationThe organic layer was filtered by means of a PTFE
6. filtrationfilter tube
7. concentrationconcentrated under reduced pressure